Apparatus for analyzing the particle size distribution of a powder sample



Feb. 17, 19.53

R. E. PAYNE 2,628,787 APPARATUS FOR ANALYZING THE PARTICLE SIZE DISTRIBUTION OF A POWDER SAMPLE Filed- Sept- 2, 1947 2 SHEETSSHEET l liill l lllllllll;

A s INVENTOR.

A Q RDBERTE.PAYNE illi/Ill Feb. 17, 1953 R. E. PAYNE 2,628,737 APPARATUS FOR ANALYZING THE PARTICLE SIZE DISTRIBUTION OF A POWDER SAMPLE Filed Sept. 2, 1947 2 SHEETS-SHEET 2 'LVAVAVAVAVJVAVAVI:

W ai y/( 0445 Fatented Feb. 1 7, 1953 UNITED s'rA'rEs ATENT OFFICE APPARATUS FOR ANALYZING THE PARTI- OLE SIZE DISTRIBUTION OF A POWDER SAMPLE Robert E. Payne, Bywoocl, Upper Darby, Pa., assignor to The Sharples Corporation, a corporation of Delaware 6 Claims.

This invention relates generally to a method and apparatus for analyzing and determining the particle size distribution of powdered or finely divided materials by indicating the rate of fall in a gaseous medium of particles of a powder sample and more particularly to feed devices for introducing the powder sample to be analyzed into the apparatus.

The presentapplication for patent is a division of my copending patent application Serial No. 768,907, entitled Sedimentation Tower, and filed August 15, 1947, now Patent No. 2,597,899, issued May 27, 1952.

A method and apparatus for determining particle size distribution of finely divided or powdered materials is known. The prior art device for such purpose employs the principles of Stokes law to determine particle size distribution by observing the rate of fall and percentage amount of particles having that rate of fall of a sample of powder initially dispersed in a liquid medium. Such liquid sedimentation devices, as they are known, are enabled to produce useful results but are not completely satisfactory in view of a number of inherent difficulties encountered when endeavoring to measure the rate of fall in a liquid medium. One difiiculty is the relatively long period of time necessary for all of the particles dispersed in a liquid medium to settle which therefore prevents a rapid determination of particle size distribution. Another difliculty with the liquid sedimentation apparatus is the tendency of the dispersed particles to aggregate into larger size units. In addition they may stick to the side walls of the liquid sedimentation tank for a time and then be released through the action of fluid currents or mechanical disturbances so as to give an incorrect value of particle size. Still another diificulty with liquid sedimentation devices for measuring particle size distribution is the disturbing effect of undesired fluid currents introduced into the liquid medium such as convection currents or currents resulting from the movements of a collecting pan or from outside vibrations affecting the liquid containing tank.

t is a principal object of this. invention to provide novel feed apparatus for introducing and dispersing in deaggregated form a powder sample into a form of gaseous sedimentation apparatus for measuring the particle size distribution of finely divided materials such as the sedimentation tower described in my copending patent application of which this application is a division. "Another object of this invention is to make possible the continuous observation of the percentage of particles having a given rate of fall under any desired conditions of fluid pressure or viscosity consistent with a desired maximum rate of fall for the largest expected particles of any powder sample.

Still another object of this invention is to pro vide an improved apparatus for the determination of particle size distribution by indicating the rate of fall and percentage of particles having that rate of fall in a gaseous medium such as air under controlled conditions of viscosity, the apparatus being relatively immune to the disturbing effects of fluid currents or vibrational influences and the difficulties arising from the aggregation or reaggregation of the particles initially dispersed in thegaseous medium before they are settled upon the collectingelement.

The gaseous sedimentation apparatus as described in the aforesaid copending patent application in its principal embodiment may be briefly described as comprising an enclosure having a vertically extending tube or tower. The enclosure may be constructed of suitable materials such as steel or the like in a manner to be substantially pressure tight. Suitable valve structures .and pressure-indicating devices may be provided in association with the enclosure and vertically extending tank to control, maintain and indicate the gaseous pressure or viscosity conditions within the enclosure either at atmospheric, subatmospheric or super atmospheric conditions. According to this invention, novel means is also provided in association with the tower to introduce and disperse within the tower in deaggregated form the sample of. powder or finely divided material to be analyzed by sedimentation within the tower in a manner not to disturb the desired condition of viscosity of the gaseous medium within the tower.

A collecting means, which may preferably be a weighing pan, is disposed in the bottom of the tower within the enclosure in a manner to receive all of the particles settling through the tower. The collecting means is fastened to one end of a lever arm which may be, if desired, pivoted at or near its center of gravity in any suitable manner such as by a substantially frictionless torsion wire or reed pivot and completely self-contained within the pressure-tight enclosure. The other or opposite endof the lever arm maybe provided with means to impose a restoring torque or counter torque on the lever arm to maintain equilibrium of the lever arm as the initial torque mam due to the weight of powder accumulating on the collecting means increases.

As more particularly described in the abovementioned copending application, the restoring torque is applied to the lever arm by electrical means so that the electrical signal necessary to produce a restoring torque sufficient to maintain equilibrium of the balance arm is proportional to the amount of powder or particle's accumulating on the collecting means. The electric signal indicating means may be positioned exteriorly of the pressure-tight enclosure and is usually calibrated arbitrarily, since the information desired to be obtained from the apparatus is of a relative nature to indicate the percentage of particles fallen upon the collecting element at any given time from zero time to the time when all particles have fallen and no further change in weight of the collecting element is observed. If desired, automatic continuous recording means of well known design may be u's'ed to record the value of the electric restoring torque signal.

In order to apply automatically the electrical restoring torque to the lever arm, in accor ance with variations in weight of the collecting means, a combined optical and photo-electric system for converting mechanical movement of the lever arm into electrical energy together with relay or amplifying means for applying such electrical energy to an electro-magnetio coil in the manner or a servo system may be used. Alternatively, means may be employed to convert the mechanical movement of the lever arm into electrical energy such as a resistance or capacity bridge, an electro-magnetic coil system, or a system of piece-electric crystals, it being understood that the electric energy thus generated or obtained is relayed to an electro-magnetic restoring torque coil in a manner to maintain the equilibrium of the lever arm as the particles collectupon the collecting means.

practicing the gaseous sedimentation method described in the aforementioned copending p'f 'tent application, the sedimentation tower is usually operated with air as the gaseous medium, although it should be apparent that other gases may be usedii desired. The temperature and pressur conditions of the gaseous medium are noted in order to determine its viscosity for use in applying the principles of the general settling law or in special cases Stokes law to t -amine the meter readings into particle size distribution; Thepressure of the gaseous medium may be controlled to provide a desired viscosity which controls the settling rate of any given powder sample to be tested. Normal temperature variations of the gaseous medium have very little effect on its viscosity and may for most practical purposes be ignored. By using the novel apparatus of this invention, the powder sample to be tested is preferably introduced and dispersed in the form of a small cloud of deaggregated particles at the top of the tower coincidental with the establishment of zero time for the observations to be recorded. If the tower is being operated under atmospheric conditions of pressure, the powder sample may be introduced and projected by'a small jet of air, although under sub-atmospheric conditions it is preferable that the powder sample be mechanically projected into the top of the tower in order to produce the desired cloud of particles at the top of the tower. If, however, the powder sample is introduced by a jet of air into the sedimentation towor under vacuum or sub-atmospheric conditions, the powder will be uniformly dispersed throughout the length of the tower and additional graphical calculation from the observed results must be made as will be later described in detail.

The meter reading at zero time is recorded and subsequent meter readings at short intervals of time from the zero time are also recorded until no further changes in the meter readings are observed, thus indicating the complete settling of all particles of the powder sample. As mentioned before, a continuous recording meter may also be used to instantaneously record meter readings versus time from zero time. In any event, the meter readings are then corrected to ZElO and normalized to thus be translated into percentage fall of the total sample of powder at any given time from zero time to the time when all particles have settled. The largest particle size settling upon the collecting element at any given time from zero time is given by Stokes law for a mospheric pressure conditions in the settling tower and by the general settling law for any pressure including atmospheric pressure when the powder sample is introduced in the form of a small cloud at the top of the tower. Stokes law is Pgt where d=particle diameter; g=acceleration of gravity; =viscosity of medium; h=height of settling column; P true density of powder material, and tztime in seconds from zero time. The general settling law that may be used for any pressure of a gaseous medium in the settling tower is go h l LOIL/ where By applying the appropriate one of the foregoinglaws to the time and percentage data obtained from the sedimentation tower as previous- 1y described, a percentage weight of particles having a particle size smaller than a given particle size may be graphically plotted over the entire percentage range of particles so as to determine the particle size distribution of finely divided or powder materials.

Further objects and advantages of this invention will be apparent with reference to the following specification and drawings in which:

Figure 1 of the drawings is a diagrammatic illustration of 'a gaseous sedimentation apparatus showing the enclosed sedimentation tower having means to introduce and project the powder sample into the top of the tower, collecting means and associated lever arm together with .the photo-electric system for translating movesedimentation tower;-

ment of the lever arm into an electrical restoring torque signal indicative of the weight of particles collected;

Figure 2 is an enlarged fragmentary partial section of the upper end of the sedimentation tower to show in detailed section one form of air feed device of the invention for projecting and dispersing the powder sample in deaggregated form within the top of the tower:

Figure 3 is a detail section of a modified for of air feed device employing a screen element for deaggregating the powder sample;

Figure 4 is a side elevation of still another form of air feed device having an adjustable slit opening through which the powder is adapted to be blown in deaggregated form into the top of the Figure 5 is anend view as seen from the bottom of Figure 4;

Figure 6 is a top plan view of the feed device shown in Figures 4 and 5;

Figure 7 is a sectional view of an alternative mechanical feed device for projecting and dispersing the powder sample in deaggregated form into the top of a sedimentation tower, the feed device being particularly suitable for use in the gaseous sedimentation tower operated under subatmospheric pressure conditions; v

Figure 8 shows a typical curve of the results obtained by a test run of a gaseous sedimentation employing the feed devices of this invention for the analysis of the particle size distribution of silica powder, and

Figure 9 is an illustration of a graphical method for computing the results recorded in the manner of'Figure 8 when obtained by operating the sedimentation tower at sub-atmospheric pressure together with air feeding of the powder sample into the tower.-

Referring to Figure 1 of the drawings wherein a gaseous sedimentation apparatus is diagrammatically shown, the completely enclosed sedimentation tower I 0 of a known height is provided and may be constructed of suitable mate'- rial, such as metal, in a manner to be pressure tight, as will be later referred to in detail. The bottom of the sedimentation tower enclosure I0 is enlarged, as shown at H, to provide space for enclosing the weighing assemblyincluding the collecting means I 2 positioned to receive the par-- ticles settling through the tower Ill, The collecting means I2 is mounted upon one end l3 of a lever arm 14 pivoted at the fulcrum [5. The opposite end.l6 of the lever arm I4 is provided with a restoring torque coil of wire I! having flexible electrical connections l8 and I9 passing through the housing I I in pressure tight relation.

The restoring torque coil I1 is positioned with its axis in an approximate horizontal plane and its coil faces between the opposed and opposite polarity pole faces of a pair of permanent magnets, one of which is shown in Figure l to have the pole faces 20 and 2|. Such an arrangement of permanent magnets and restoring torque coil functions as a servo system electric motor, as should be well understood. A light reflecting mirror 22 is mounted upon the lever arm 14 in the vicinity of the fulcrum IE to be deflected with the lever arm I4 as it is moved toward either of f the dotted line positions in response to the application of forces on the lever arm as willbe described. It should be understood that the dotted line positions of the lever arm l4 are greatly exaggerated for purposes of illustrating the invention; since the amount of deflection of the lever arm 14, due to the accumulation of particles on the collecting means 12 is practically imperceptible except as may be detected by an automatically responsive servo system. Further-- more, the servosystem to be described is adapt-- ed to supply an electrical signal to the electro magnetic coil ll in a manner to'apply a restor-- ing torque to maintain equilibrium of the lever arm M as the weight of particles on the collecting means [2 increases and thus further limits the movement of the lever arm to be almost imperceptible.

In the diagrammatic illustration of one formof the lever arm 14 upon the photo-electric assembly 30. The relative positions of the light source 25 and the reflecting mirror 22 carried by the lever arm I4 may be such that when the lever arm I4 is in the horizontal equilibrium position, the reflected light beam 21 is evenly divided by the prisms 3| and 32 between the photo-electric cells 33 and 34. Upon movement of the equi-- librium position for the lever arm [4 to a position other than the horizontal position, with such relative positioning of the light source 25 and reflecting mirror 22, either the photo-electric cell 34 or 33 will receive more light than the other as should be readily understood.

The photo-electric cells 33 and 34 are connected in a circuit with their anodes connected together and to the positive terminal 35 of a battery 36 or other suitable voltage source. The negative terminal of the battery 36 is grounded and connected to the mid point of a voltage divider connected across the respective cathodes of photo-electric cells 33 and 34. Thus, when the lever arm I4 is in the horizontal equilibrium position, the potentials at the respective cathodes of the photo-electric cells 33 and 34 may be equal so that the potentials in lines 31 and 38 connected to the input terminals of a balanced amplifier 39 are also equal with respect to ground. The balanced amplifier may be of any well-known type which will produce a voltage output of a polarity and amplitude relative tothe potential difference in lines 31 and 38 as applied to its input terminals. The output voltage from the balanced amplifier 39 is connected by lines 40 and 4| to the electromagnetic coil l1 in a manner to create a magnetic field to interact with the field of the permanent magnets and apply a restoring torque on the end of the lever arm M to maintain its equilibrium as it'is tended to move by the accumulation of particles on the collecting means 12. In effect, the amplifier 39 functions as an impedance matching device between the relatively high impedance of the photo cells and the low impedanceof the restoring torque coil and. supplies the necessary restoring torque power.

Although the electro-optical servo system as diagrammatically shown and described thus far, is. of the type in which the lever arm l4 may be balanced in the horizontal equilibrium position without the application of any electromagnetic restoring torque or energy in the coil ll,1it should be apparent that the system is not necessarily limited to such an arrangement. For example, the fulcrum point l5 may be located ata position-other .than just above the center o-f gravity for; the lever-18mm M, in which. case the servo system maybe modified; asshouldbe readily understood; to: provide acontinuous; restoring torque through the. medium. of the electro-magnetic coil 11 and associated; perma: nent magnets to maintain the lever arm H1 in a desired equilibrium. position, at' the: start of a test run and during the subsequent accumu: lation of powderupon the collecting means. l2;

A meter t2 may be provided inv the outputcircuit of the amplifier electro-magnetic restoring torque coil; IT to .indicate the electrical energy proportional to such restoring torque, automaticallyobtained-inv re.-. sponse to the tendency of" movement of' the lever armit: andthu'sindicate the amount of.

powder collected; onthe collecting. meansl2.v The; meter 42 may. be. of the-. micro -ammetertype connected in a. manner to measure the current, but it; should be. understood thatany type of device. connected. to. measure electric current or voltagemay beusedto indicate the restoring torque; energy. meter may be.- calibrated arbitrarily. fromzero to 100, since its deflection. is. only sin-arbitrary indication of theamount .or percentage weight of particles collected on. the collecting-means: 12 at any. interval of 'time. from zero timeto the time. when all particles have fallen. The meter may, alsobe calibrated. directly in milligrams weight on collecting means, if so dersirecl. A continuous time .1 recording meter of" known design (not shown) may also be used in place of the meter 42, ashas been previously mentioned At the top of the sedimentation tower-'lU-as" diagrammatically shown in Figure 1, a powder feed means fiilz-for introducing and dispersingin deaggregated form a: sample-of powder to be analyzed is provided. The feed means 59, ac-

cording to this invention, may have-a number of'modified structural forms and arrangements such as shown in detail byFigures- 2 through '7 ofthe drawings, and, as'shown diagrammatically to be passed. through the valve :52into the pipe.

line 53. A smallt'volume of air contained inthe small pressure chamber 54 under pressure may then be released by closing the valve 52 and opening the valve 55 to project the powder sample in the pipe line 53 through the slit orifice of the feed device 5%] into the top of the sedimentation towerl0 to-form asmall cloud of dispersed particles. The feed device 56 is preferably provided with an orifice having a size equal to the largest particle size expected to be present in the powder sample andfurther having a structure such as to cause deaggregation of the powder sample as .it is blown into the top of the sedimentation tower It.

It may be desirable to operate the sedimentation tower under conditions of sub-atmospheric pressure in which case the valves 55, 51, 53 and pump fiiimaybe suitably manipulated in a known manner to control the pressure within the sedimentation tower H], as indicated by any. standard type of pressure or vacuum gauge 60;

39 connected. to the,

In. any event, the

The sample of powder to be In place of the simple arrangement of valves mentation-;tower.- enclosure. l0; and: the. enlarged bottom enclosure H.

The operation of the gaseous sedimentation system thus far described is as follows. A sample of powder is blown into the top of the. sedimentation tower 46' through the powder feed device 53; as previously described. Zero time for the observations to be recorded is established co-incident with the time of introduction of the powder sample into the top of the tower. In accordance with the principles of the well-known settling law, the largest particles ofpowder will reach the-collecting device l2 at the bottom of the tower it. in a very short interval of time after zero time. Prior to the introduction of the powder sample into the top of. thetowenthe lever arm I4 is adjusted in amanner: such as referredto in detail in the aforesaid'copending patent application, to a condition of equilibrium with the reflected light distributed upon the photo cells 33 and i l to. cause a full-scale or approximately full-scale meter deflection by the meter #32 and a consequent amount of electromagnetic restoring torque by the coil ll assisting in maintaining the equilibrium of 'the'lever arm Ml. As the first particle is collected bythe collectingdevice I2, the equilibrium of the lever arm I l tends to be disturbed, causing a, shift in light distribution on the photo cells 33 and also that the electrical energy output of the balanced amplifier 39 is changed to produce a corresponding change in the restoring torque of coil 'li to maintain the lever arm i l in equilibrium for the-new condition of weight on the collecting device 12. The change in electrical energy is indicated by the meter t2 and may be-recorde'd along with the time lapse from the zero time at which the meter-change occurs. Subsequent particles fall'- ing upon the collecting device l2cause subsequent changes in the meter readings-and restoring torque and by plotting the meter readings versus time and normalizing the meter readings, such asin a manner to be hereinafter described, apercentage weight indication-of particles fallingupon the collecting device !2 will be obtained.

At some subsequent time from the-zero time, a

form of air-operated feed device for introducing and dispersing in deaggregated form a sample of powder to analyzed, is shown in detail.

The top of the cylindrical sedimentation tower" Hl is provided with a flange lflfl'upon which is seated a disc shaped end piece HJI. To maintain the pressure tight relation within the tower l0 a-rubber gasket H 2 may be provided and a plurality of bolts such as liiii'and lll lmay be. em-.

ployed to assure a tight seating of the end piece [01- against the gasket H712 and flange lilo. A tubular conduit ice passes throughthe end piece l0! and is welded thereto in pressure tight. rela tion.. The conduit N15 is adapted to support Withinthe upper end of the sedimentation tower Hi the feed deviceassembly i H3 .Thefeed-device H6 is comprisedofa metallic blockor body-member'l ll having the axial bore l lienlarged atits lower. endato. form a conical;

opening II3 with the large end of the cone at the surface of the block and facing the interior of the tower i3. Within the bore H3 and conical opening I I3 is positioned a closely fitting plug II4 of similar contour which may, if desired, be of slightly less dimensions. The plug H4 is held in assembled relation to the block II I by the threaded nut II5 carried by the bracket IIS. By adjusting the threaded nut II5 to move the plug II 4 lengthwise of the conical opening II3, the dimensions of the slit orifice formed between the opposing conical surfaces of the conical opening I I3 and the plug I I4 may be correspondingly adjusted. The powder sample and accompanying air blast from the air storage chamber 54 shown in Figure 1 of the drawings is conveyed by gas pressure through the supporting conduit I05 into the passage-way Ill, bored in the block I I I to connect with the orifice between the conical surface H3 and plug II 4. In order to prevent the blast of powder and air from escaping around the upper end of the block III, a packing nut H8 is provided. I In employing this form of feed device, the nut H5 is adjusted to provide a clearance or orifice between the opposing conical surfaces of the feed device equal to or slightly larger than the largest expected particle size of the powder sample. The arrangement of conical surfaces within the feed device together with the use of an air blast to blow the powder through the feed device is effective to deaggregate and thoroughly disperse the powder sample in the form of a cloud within the top of the sedimentation tower I!) by breaking up the particle aggregates larger than the largest expected particle size equivalent to the width of the narrow dimension of the slit orifice.

An alternative type of feed device is shown in Figure 3 of the drawings. A mixture of air and powder sample is conveyed through the inlet tube I05 against a fine mesh screen I 2| at an angle to the screen such that the smallest expected particle size cannot pass through the screen without striking a screen wire or cross member of the mesh. Therefore all particles and aggregates of particles must strike a cross wire of the screen I2I and be deflected and deaggregated to pass through the screen at right angles to the plane of the mesh screen into theoutlet tube I22 and the top of the tower III. The mesh screen I2I is interposed between the inlet tube I05 and the outlet tube I22 and may be clamped between.

a pair of plates I23 and I24 having a sealing gasket I25 to prevent the escape of air and powder around the edges of the plates I23 and I24.- Such form of feed device is particularly suitable for use in feeding powder samples containing a large percentage of aggregates which must be deaggregated to prevent clogging in the small orifice feed device. Deaggregation is necessary in order to obtain accurate analytical results from the sedimentation tower. The mesh screen may preferably be of 200;mesh size, al

though such size is not a limitation since most of the smaller mesh screens presently available have screen openings considerably larger than the largest particle size to be passed in a given powder sample.

Yet another form of airfeed device is shown in Figures 4 through 6 of thedrawings. This form of air feed device may also be termed a slit feed, the width of the narrow dimension of the slit being determinate of the maximum particle size fedthrough the device. H15, in which is onveyed the mixture of sample The conduit powder and air under pressure, is clamped at I3I between the plate members I32 and I33 having cut-out or depressed portions in their opposed surfaces to form the passage-way I34. The passage-way I34 narrows down to a slit I35 at one end of the plates I32 and I33, as shown in Figures 4 and 5 of the drawings. The edges of the depressed surfaces and passage-way I35 are defined by the gaskets I36 and I3! which prevent the powder and air under pressure from escaping between the two plates I32 and I33 except at the slit opening I35. The width of the narrow dimension of the slit I 35 is determined by the spacing between the opposed plates I32 and. I33 which are tightly clamped together at the end adjacent the feed conduit I35 by means of the bolts I38--I4I. At the end of the plates I32 and I33 adjacent the slit opening I33, the spacing between the plates is determined by the adjustment of the studs I42 and I43. Studs I42 and IE3 are provided with differentially threaded sections at each end, one section engaging corresponding threads in the lower plate I33 and the other section engaging a threaded collar I 44 or I45 carried by the upper plate I32. .The threaded sections at each end are in the same direction but one end has 50 threads per inch while the other end has 51 threads per inch giving a very high mechanical amplification of slit motion. Each of the studs I42 and I43 have keyed thereon a worm wheel I46 and I II engaging worms I48 and I 49 which may be rotated by the keyed shafts I50 and I5I. It should be apparent that rotation of either worm I48 or I49 will adjust the spacing between the opposed plate surfaces I32 and I 33 at the slit opening and thus regulate the width of the slit opening and the maximum particle size to be passed through the opening. The passage-way I35, shaped as shown in the dotted lines of Figures 4 to 6, is effective to disperse and deaggregate the powder sample in the form of a cloud within the top of the sedimentation chamber.

In the powder feed devices of this invention having slit orifices through which the powder sample is projected by a jet of air, examples of which have been described in connection with Figures 2 and 4 to 6 of the drawings, very effective deaggregation of the powder sample is primarily due to a viscous sheer force upon the particles asthey pass through thehigh velocity stream of air in the slit which therefore may be larger in its narrow dimension than the largest expected particle size. The above will be better understood when it is pointed outthat the move-; ment of air in the center of the slit or orifice is of very high velocity while the air movement at the side walls of the orifice is substantiallyzero;

All of the forms of feed devices of this invention thus far described in connection with Figures 2 to 6 of the drawings employ a jet of air. to 1 project the powder sample into the top of the sedimentation tower. v Under certain conditions of operation it might be undesirable to introduce the powder sample. by means of a jet of air. For

example, when the sedimentation tower-is to be operated under conditions of vacuum, it is apparent that if the powder sample is introduced into the tower by. means of a jet of air, the particles would-uniformly distribute themselves throughout the tower from top to bottom at the instant of zero time beforesettling of the par ticles. While such a distribution would not pre- 1 vent a determination of the particle size distribution, it would necessitate a graphical computation ll of the results obtainedwhen the particles are so uniformly distributed throughout the tower instead of dispersed in the ,form of a cloud at the top of the sedimentation tower.

An alternative mechanical feed device may be used to projectthe powder sample into the top of the tower in .the form of acloud of dispersed and deaggregated particles, without the introduction of an air blast into the tower and regardless of the pressure conditions within the tower. Such a mechanical form of feed projecting device is shown in Figure 7 of the .drawings. A cylindrical tube or cylinder I63 is supported upon an arm ifii welded to the inner wall of the sedimentation tower it and is provided with an open end upwardly communicating with the interiorof the tower it. Since the feed device is adapted to project the powder sample upward, it may be positioned at any suitable point within the sedimentation tower Hi beneaththe upper end of the tower. Reciprocallymounted within the cylinder I6!) is a piston .member I62 having a flanged latching surface J63 .on its .under side. Piston rings (not shown) may be provided .to maintain a pressure tight fit between the piston .152 and the inner cylinder walls of the cylinder Hit. A pivoted latch member .164 normally engages the latch flange I63, .asshown, to prevent the piston IBZ-from moving upward within the cylinder .169.

A feed tube 165 .is adapted toproject through the outer wall .of the sedimentation tower .iil with :a flexible bellows or seal 1 6.8 and suitable valves I6? and 1.68 ,of the pressure locking type are provided to permit a powder .sample to be introduced through the feed tube 155 onto the upper surface of thepiston I552 without disturbing .a pressure condition within the tower l0, as should be readily understood. The bottom end of the feed tube I65 is passed within the cylinder I60 above the upper surface of the piston I162 by means of the flexible bellows or seal 860. The provision of the .flexible bellows 166 and 169 enables the feed tube Ifil to be moved inward to the dotted line position to deposit the powder sample upon the center of the upper surface of the piston I62, after which the feed tube may be withdrawn to thesolid line position to provide clearance for the piston I62 when it is moved upward within .the cylinder 160.

The lower end of .the cylinder 160 carries a compression spring I'll) seated against an adjustable .spring tensioning plug 11 threaded within the bottom portion of the cylinder .ifill. The upper end of the spring 110 seats against a disc portion H2 of a flexible bellows or seal 1.73 connected between the inner walls of the cylinder 1.60. The disc member I12 also carries a trigger element 114 normally engaging, as shownin the drawings, the dependent portion of the latch member 1.64 and preventing the latch member J64 from pivoting in a clockwise .direction to release the piston I62 .f r axial movemen upward within the cylinder L60. A conuit 1. .5 is provided with associated valves H5 and I'll toadmit air under pressure into the cylinder chamber I18 defined by the bottom surface of the p n I62 and the flexible bellows and disc member H3 and 112, respectively. When the valve H6 is manipulated to admit .air under pressure into the chamber 118, the bellows H3 is movfid a ainst the force of the compression spring H0 until the .air pressure-exceeds the tension of the spring and the trigger member 576 is moved to release the latch 1.64- for pivotal movement in a clockwise direction. The-air pressure within the chamber -Hfl'thus controlled by the tension of the spring H9 :is .then operative to force the piston I62, now released for axial movement .by the clockwise pivotal movement of the latch 5%, to move axially upward within the cylinder see with considerable velocity. At the upper end of the cylinder 180, the piston strikes the rubber gasket-andshock absorbingring 88 and fiings the powder sample on .its upper surface upward through the mesh screen iSl toward the top of the tower. The mesh screen it! is supported .on anumber of bracketarms, such as l82 and lfitandiunctions to'deaggregate the powder sample as it is projected upward. into the top of the sedimentation tower H]. By ciosing valve Iliiand opening valve i '1? the-air pres sure within the chamber 118 may be released to allow the piston I 62 :to .fall .by gravity andreset the trigger mechanism including the pivoted latch 5 3 for a subsequent ieed of a powder sample.

The following results may be given as an example .of one test .run .of gaseous sedimentation apparatus when employing an air feed device of this invention, such as shown and described in connection with Figure 20f the drawings. The results tabulated below were :obtained by initially adjusting :the position of the lever'arm iii to causefullscale meter=deflection. The test run was made .atatmosphericpressure and was continued .for a time duration of 85,800 seconds (longer than usually needed for most powder samples) .at which time no further meter =defiection was observed, thus indicating complete settling of allpowderparticles. The meter .readings were corrected tovzero andnormalized to indicate percentage weight, asst-Town in the taou lationslistecl below. The maximum particle size for listedpercenta-ge 'weightsrat specified time in tervals from zero time were computed by Stokes law, since the gaseous medium in the tower was maintained at atmospheric pressure during the test run.

Divide by Subtract 93.7 m pute bi- Meter to 6.3 to Corre okes Law Time, secon Reading Correct 'to 100% plan i ter (N ormall a Zatio -m1c1ons Percent wt finer than (i 100 .100

a given time lapse from zero time to use the general settling law instead of the simplified Stokes law, which is true only for atmospheric conditions of pressure. It is preferable to employ the mechanical feed device shown and described in connection with Figure 7 of the drawings when operating a gaseous sedimentation tower under sub-atmospheric conditions of pressure so that a cloud of dispersed particles of the powder sample may be formed at the top of the tower. However, when operating the tower under sub-atmospheric conditions of pressure, an air feed device may be employed in which case the powder sample is substantially uniformly distributed throughout the settling tower coincident with zero time and therefore making it necessary to compute and correct the results for such particle distribution graphically. In Figure 9 of the drawings the graphical computation and correction method is illustrated where in the diameter of the particles as determined from the general settling law is plotted along the abscissa starting with zero at the left and the arbitrary corrected meter readings for the corresponding particle sizes are plotted along the ordinate starting with zero meter reading at the bottom. The true percentage values may then be obtained by constructing tangents to the curve representing pairs of meter readings and diameters. The intercept of the tangent on the ordinate will then indicate the true percentage weight of powder having the particle size finer than the size d indicated at the tangent point on the curve. For example, at a point P: on the curve representing a particle size (is a tangent is drawn to intercept the axis at the point R3. Percentage weight We will then be obtained by the following formula:

The percentage weight and particle size may then be graphically plotted as previously shown in Figure 8 of the drawings.

While the feed devices of this invention have been particularly described in connection with their use for introducing particles of the powder sample into the tower of gaseous sedimentation apparatus, it should be understood that the feed devices are not necessarily limited to such application. For example, the feed devices of this invention may be used to advantage under any circumstances where it is desired to produce a cloud of dispersed and deaggregated particles of a powder sample in a fluid medium. Such a cloud of particles might be produced in atmosphere by the feed devices of this invention, and the particles settling through the atmosphere may be collected on microscope slides for microscopic examination and counting in order to analyze a particle powder sample.

It should be obvious that various modifications of the gaseous sedimentation feed devices and apparatus of this invention Will occur to those skilled in the art without departing from the spirit and scope of the appended claims.

I claim:

1. In an apparatus for analyzing the particle size distribution of a powder sample, a vertical gas-containing sedimentation tower, a powder injection conduit extending into the upper part of said tower, a powder supply; conduit external to said tower and extending upward from said first conduit intermediate the ends thereof, the upper end of said supply conduit being open to receive a small quantity of powder constituting the sample to be analyzed, a valve in said supply conduit which may be opened to supply the powder sample to said injection conduit, said valve being thereafter closed to preclude passage of air, a source of pressurized gas connected to the end of said injection conduit external to said tower, a normally-closed valve in said injection conduit between said source and said supply conduit, whereby opening of the latter valve causes a blast of pressurized gas to impinge against the powder sample held by said injection conduit and efiects forceful delivery of the powder sample through said injection conduit to the upper part of said tower, and means at the delivery end of said injection conduit within said tower for dispersing and deaggregating the powder sample, so as to form a cloud of powder particles free to gravitate downward within the sedimentation tower.

2. In an apparatus for analyzing the particle size distribution of a powder sample, a vertical gas-containing sedimentation tower, a powder injection conduit extending into the upper part of said tower, hopper means external to said tower and extending upward from said injection conduit intermediate the ends thereof, whereby a small quantity of powder constituting the sample to be analyzed may be introduced into said conduit through said hopper means, means for effecting pressure-tight closure of said hopper means after introduction of the powder sample, a source of pressurized gas connected to the end of said injection conduit external to said tower, a normally-closed valve in said injection conduit between said source and said hopper means, whereby opening of said valve causes a blast of pressurized gas to impinge against the powder sample held by said injection conduit and effects forceful delivery of the powder sample through said injection conduit to the upper part of said tower, and means at the delivery end of said injection conduit within said tower for dispersing and deaggregating the powder sample, so as to form a cloud of powder particles free to gravitate downward within the sedimentation tower.

3. Apparatus according to claim 2, wherein said dispersing and deaggregating means comprises a body member having a vertical downwardly flared conical opening, and a cone member positioned within said opening and forming with said body member a narrow passage or orifice to which the powder is supplied.

4. Apparatus according to claim 3, wherein said cone member is adjustable axially to vary the size of said passage or orifice.

5. Apparatus according to claim 3, wherein said members are constructed to form a vertical extension of the narrow passage or orifice so as to emit the powder particles vertically downward.

6. Apparatus according to claim 2, wherein said dispersing and deaggregating means comprises a fine mesh screen arranged in the path of travel of the forcefully delivered powder.

ROBERT E. PAYNE.

(References on following page) REFERENCES CITED The following references are of record in the file of this patent: V

UNITED STATES PATENTS Number Name Date Hofimann Sept. 12, 1933 Andersen May 18, 1937 Number 16 Name Date Hammack -1. May 17, 1938 Schanz 1 June '7, 1938 Berry Feb. 24, 1942 Anderson et a1 July 4, 19 Trist Nov. 13, 1945 Stephanofi Dec. 31, 1946 Ca-kebrea'd May 2'7. 194? 

